data_shelx _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H15 N O2, Pd, (C6 H5)3 P' _chemical_formula_sum 'C32 H30 N O2 P Pd' _chemical_formula_weight 597.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1130(9) _cell_length_b 11.3390(11) _cell_length_c 13.8100(12) _cell_angle_alpha 109.376(3) _cell_angle_beta 105.198(4) _cell_angle_gamma 93.408(3) _cell_volume 1282.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13035 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 75.78 _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_F_000 612 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.067 _exptl_absorpt_coefficient_mu 6.669 _shelx_estimated_absorpt_T_min 0.364 _shelx_estimated_absorpt_T_max 0.664 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.459 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'sealed microfocus tube' _diffrn_measurement_device_type 'Agilent SuperNova with AtlasS2 CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15182 _diffrn_reflns_av_unetI/netI 0.0160 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.556 _diffrn_reflns_theta_max 76.893 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5283 _reflns_number_gt 5220 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _publ_section_references ; CrysAlisPro. Agilent Technologies (2013). Agilent Technologies UK Ltd., Oxford, UK, SuperNova CCD System, CrysAlicPro Software System, 1.171.37.31 Palatinus, L. and Chapuis, G. (2007). Superflip. J. Appl. Cryst. 40, 786-790. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (2015). SHELXL-2014/7. Acta Cryst., C71, 9-18. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrysAlisPro V 1.171.37.31, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro V 1.171.37.31, Agilent Technologies' _computing_data_reduction 'CrysAlisPro V 1.171.37.31, Agilent Technologies' _computing_structure_solution ; SUPERFLIP. Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790. ; _computing_structure_refinement 'Shelxl-2014/7, Sheldrick, G. M.' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material 'Shelxl-2014/7, Sheldrick, G. M.' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.0035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5283 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1077(2) 0.24747(18) 0.08795(15) 0.0227(4) Uani 1 1 d . . . . . C2 C -0.0473(2) 0.18472(19) 0.05003(16) 0.0271(4) Uani 1 1 d . . . . . H2 H -0.0753 0.1247 0.0790 0.032 Uiso 1 1 calc R U . . . C3 C -0.1575(2) 0.2086(2) -0.02724(15) 0.0279(4) Uani 1 1 d . . . . . H3 H -0.2604 0.1662 -0.0495 0.033 Uiso 1 1 calc R U . . . C4 C -0.1208(2) 0.2936(2) -0.07338(16) 0.0305(4) Uani 1 1 d . . . . . H4 H -0.1978 0.3100 -0.1266 0.037 Uiso 1 1 calc R U . . . C5 C 0.0282(2) 0.3536(2) -0.04087(16) 0.0287(4) Uani 1 1 d . . . . . H5 H 0.0537 0.4105 -0.0735 0.034 Uiso 1 1 calc R U . . . C6 C 0.1455(2) 0.33362(17) 0.03957(14) 0.0221(4) Uani 1 1 d . . . . . C7 C 0.2973(2) 0.40127(17) 0.06569(14) 0.0215(3) Uani 1 1 d . . . . . H7 H 0.3090 0.4611 0.0326 0.026 Uiso 1 1 calc R U . . . C8 C 0.6810(2) 0.39697(18) 0.17516(15) 0.0237(4) Uani 1 1 d . . . . . H8 H 0.6887 0.3237 0.1128 0.028 Uiso 1 1 calc R U . . . C9 C 0.6656(2) 0.35494(17) 0.26832(14) 0.0199(3) Uani 1 1 d . . . . . C10 C 0.7949(2) 0.27776(19) 0.28733(16) 0.0251(4) Uani 1 1 d . . . . . H10A H 0.7983 0.2150 0.2185 0.030 Uiso 1 1 calc R U . . . H10B H 0.7808 0.2327 0.3354 0.030 Uiso 1 1 calc R U . . . C11 C 0.9450(2) 0.3787(2) 0.34137(17) 0.0293(4) Uani 1 1 d . . . . . H11A H 0.9962 0.3829 0.4154 0.035 Uiso 1 1 calc R U . . . H11B H 1.0185 0.3601 0.2987 0.035 Uiso 1 1 calc R U . . . C12 C 0.8837(2) 0.50107(19) 0.34172(16) 0.0283(4) Uani 1 1 d . . . . . H12 H 0.9551 0.5802 0.3934 0.034 Uiso 1 1 calc R U . . . C13 C 0.8290(2) 0.49531(19) 0.22464(16) 0.0284(4) Uani 1 1 d . . . . . H13A H 0.8074 0.5787 0.2216 0.034 Uiso 1 1 calc R U . . . H13B H 0.9068 0.4675 0.1872 0.034 Uiso 1 1 calc R U . . . C14 C 0.7288(2) 0.48107(18) 0.36437(15) 0.0262(4) Uani 1 1 d . . . . . H14A H 0.7415 0.4714 0.4346 0.031 Uiso 1 1 calc R U . . . H14B H 0.6664 0.5484 0.3585 0.031 Uiso 1 1 calc R U . . . C15 C 0.2792(2) 0.11251(17) 0.34545(15) 0.0202(3) Uani 1 1 d . . . . . C16 C 0.1629(2) 0.03363(18) 0.25418(16) 0.0247(4) Uani 1 1 d . . . . . H16 H 0.1817 0.0056 0.1863 0.030 Uiso 1 1 calc R U . . . C17 C 0.0204(2) -0.0041(2) 0.26179(19) 0.0304(4) Uani 1 1 d . . . . . H17 H -0.0574 -0.0591 0.1995 0.037 Uiso 1 1 calc R U . . . C18 C -0.0090(2) 0.0380(2) 0.3597(2) 0.0348(5) Uani 1 1 d . . . . . H18 H -0.1072 0.0127 0.3646 0.042 Uiso 1 1 calc R U . . . C19 C 0.1048(3) 0.1171(2) 0.4507(2) 0.0356(5) Uani 1 1 d . . . . . H19 H 0.0841 0.1462 0.5180 0.043 Uiso 1 1 calc R U . . . C20 C 0.2498(2) 0.15430(19) 0.44415(16) 0.0264(4) Uani 1 1 d . . . . . H20 H 0.3279 0.2079 0.5069 0.032 Uiso 1 1 calc R U . . . C21 C 0.51676(19) 0.00811(16) 0.26265(14) 0.0178(3) Uani 1 1 d . . . . . C22 C 0.5045(2) -0.09126(17) 0.29999(15) 0.0216(3) Uani 1 1 d . . . . . H22 H 0.4711 -0.0792 0.3618 0.026 Uiso 1 1 calc R U . . . C23 C 0.5410(2) -0.20759(18) 0.24716(16) 0.0253(4) Uani 1 1 d . . . . . H23 H 0.5339 -0.2748 0.2732 0.030 Uiso 1 1 calc R U . . . C24 C 0.5880(2) -0.22577(18) 0.15622(16) 0.0257(4) Uani 1 1 d . . . . . H24 H 0.6121 -0.3058 0.1198 0.031 Uiso 1 1 calc R U . . . C25 C 0.6000(2) -0.12823(18) 0.11810(15) 0.0237(4) Uani 1 1 d . . . . . H25 H 0.6327 -0.1411 0.0560 0.028 Uiso 1 1 calc R U . . . C26 C 0.56404(19) -0.01141(17) 0.17109(14) 0.0196(3) Uani 1 1 d . . . . . H26 H 0.5717 0.0555 0.1448 0.023 Uiso 1 1 calc R U . . . C27 C 0.5909(2) 0.23089(16) 0.46235(14) 0.0188(3) Uani 1 1 d . . . . . C28 C 0.6990(2) 0.17107(17) 0.51261(14) 0.0208(3) Uani 1 1 d . . . . . H28 H 0.7100 0.0869 0.4748 0.025 Uiso 1 1 calc R U . . . C29 C 0.7906(2) 0.23475(19) 0.61811(15) 0.0253(4) Uani 1 1 d . . . . . H29 H 0.8642 0.1938 0.6522 0.030 Uiso 1 1 calc R U . . . C30 C 0.7753(2) 0.35766(19) 0.67376(15) 0.0264(4) Uani 1 1 d . . . . . H30 H 0.8382 0.4007 0.7458 0.032 Uiso 1 1 calc R U . . . C31 C 0.6688(2) 0.41747(18) 0.62468(15) 0.0269(4) Uani 1 1 d . . . . . H31 H 0.6583 0.5017 0.6628 0.032 Uiso 1 1 calc R U . . . C32 C 0.5772(2) 0.35429(17) 0.51952(15) 0.0233(4) Uani 1 1 d . . . . . H32 H 0.5039 0.3959 0.4860 0.028 Uiso 1 1 calc R U . . . N1 N 0.41839(17) 0.38664(14) 0.13062(12) 0.0196(3) Uani 1 1 d . . . . . O1 O 0.20217(15) 0.22280(14) 0.16435(11) 0.0280(3) Uani 1 1 d . . . . . O2 O 0.55524(15) 0.46210(12) 0.14244(11) 0.0247(3) Uani 1 1 d . . . . . Pd1 Pd 0.43806(2) 0.28104(2) 0.22404(2) 0.01601(5) Uani 1 1 d . . . . . P1 P 0.46151(5) 0.15972(4) 0.32603(3) 0.01610(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0208(8) 0.0267(9) 0.0215(8) 0.0091(7) 0.0065(7) 0.0071(7) C2 0.0252(9) 0.0299(10) 0.0268(9) 0.0107(8) 0.0083(8) 0.0043(8) C3 0.0206(9) 0.0344(10) 0.0233(9) 0.0051(8) 0.0046(7) 0.0043(8) C4 0.0258(10) 0.0404(11) 0.0230(9) 0.0122(8) 0.0015(8) 0.0083(8) C5 0.0315(10) 0.0341(11) 0.0243(9) 0.0149(8) 0.0079(8) 0.0098(8) C6 0.0246(9) 0.0239(9) 0.0187(8) 0.0071(7) 0.0077(7) 0.0083(7) C7 0.0288(9) 0.0208(8) 0.0190(8) 0.0097(7) 0.0096(7) 0.0079(7) C8 0.0241(9) 0.0254(9) 0.0258(9) 0.0121(7) 0.0104(7) 0.0046(7) C9 0.0184(8) 0.0210(8) 0.0205(8) 0.0082(7) 0.0058(7) 0.0011(7) C10 0.0222(9) 0.0291(10) 0.0274(9) 0.0134(8) 0.0091(7) 0.0043(7) C11 0.0214(9) 0.0380(11) 0.0300(10) 0.0155(9) 0.0066(8) 0.0021(8) C12 0.0257(9) 0.0289(10) 0.0278(10) 0.0084(8) 0.0076(8) -0.0031(8) C13 0.0262(9) 0.0298(10) 0.0319(10) 0.0143(8) 0.0098(8) 0.0006(8) C14 0.0264(9) 0.0256(9) 0.0241(9) 0.0061(8) 0.0083(7) 0.0001(7) C15 0.0202(8) 0.0205(8) 0.0273(9) 0.0137(7) 0.0117(7) 0.0088(7) C16 0.0227(9) 0.0243(9) 0.0309(10) 0.0132(8) 0.0099(8) 0.0056(7) C17 0.0205(9) 0.0304(10) 0.0459(12) 0.0213(9) 0.0087(8) 0.0057(8) C18 0.0252(10) 0.0383(11) 0.0607(14) 0.0321(11) 0.0248(10) 0.0144(9) C19 0.0401(12) 0.0405(12) 0.0477(13) 0.0264(10) 0.0319(10) 0.0191(10) C20 0.0295(10) 0.0276(9) 0.0305(10) 0.0149(8) 0.0159(8) 0.0102(8) C21 0.0157(7) 0.0173(8) 0.0196(8) 0.0050(6) 0.0056(6) 0.0033(6) C22 0.0232(8) 0.0209(9) 0.0230(8) 0.0087(7) 0.0094(7) 0.0046(7) C23 0.0265(9) 0.0202(9) 0.0312(10) 0.0103(7) 0.0100(8) 0.0057(7) C24 0.0264(9) 0.0193(8) 0.0289(9) 0.0035(7) 0.0099(8) 0.0078(7) C25 0.0232(9) 0.0231(9) 0.0239(9) 0.0044(7) 0.0106(7) 0.0043(7) C26 0.0188(8) 0.0193(8) 0.0208(8) 0.0071(7) 0.0068(7) 0.0028(6) C27 0.0198(8) 0.0202(8) 0.0186(8) 0.0075(7) 0.0086(7) 0.0039(6) C28 0.0209(8) 0.0218(8) 0.0238(9) 0.0111(7) 0.0092(7) 0.0057(7) C29 0.0211(8) 0.0336(10) 0.0253(9) 0.0163(8) 0.0061(7) 0.0048(7) C30 0.0260(9) 0.0331(10) 0.0181(8) 0.0088(7) 0.0057(7) -0.0038(8) C31 0.0350(10) 0.0232(9) 0.0223(9) 0.0047(7) 0.0128(8) 0.0037(8) C32 0.0285(9) 0.0225(9) 0.0214(9) 0.0095(7) 0.0085(7) 0.0086(7) N1 0.0220(7) 0.0191(7) 0.0203(7) 0.0089(6) 0.0082(6) 0.0032(6) O1 0.0187(6) 0.0371(8) 0.0332(7) 0.0225(6) 0.0038(5) 0.0020(5) O2 0.0234(6) 0.0245(6) 0.0302(7) 0.0155(6) 0.0075(5) 0.0017(5) Pd1 0.01736(7) 0.01598(7) 0.01631(7) 0.00688(5) 0.00606(5) 0.00389(5) P1 0.01755(19) 0.01602(19) 0.01719(19) 0.00686(16) 0.00757(16) 0.00498(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.297(2) . ? C1 C2 1.422(3) . ? C1 C6 1.426(3) . ? C2 C3 1.372(3) . ? C2 H2 0.9500 . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.369(3) . ? C4 H4 0.9500 . ? C5 C6 1.414(3) . ? C5 H5 0.9500 . ? C6 C7 1.435(3) . ? C7 N1 1.285(2) . ? C7 H7 0.9500 . ? C8 O2 1.453(2) . ? C8 C13 1.537(3) . ? C8 C9 1.548(2) . ? C8 H8 1.0000 . ? C9 C10 1.528(2) . ? C9 C14 1.543(2) . ? C9 Pd1 2.0404(17) . ? C10 C11 1.565(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.525(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.540(3) . ? C12 C14 1.544(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.390(3) . ? C15 C16 1.397(3) . ? C15 P1 1.8282(18) . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.379(3) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.398(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.395(2) . ? C21 C22 1.396(2) . ? C21 P1 1.8195(17) . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(2) . ? C27 C28 1.395(2) . ? C27 P1 1.8168(18) . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 C31 1.378(3) . ? C30 H30 0.9500 . ? C31 C32 1.387(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? N1 O2 1.4099(19) . ? N1 Pd1 2.0149(15) . ? O1 Pd1 2.0682(13) . ? Pd1 P1 2.2549(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 117.37(17) . . ? O1 C1 C6 125.53(17) . . ? C2 C1 C6 117.09(17) . . ? C3 C2 C1 121.77(19) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 121.02(19) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.91(18) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.24(19) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 118.94(18) . . ? C5 C6 C7 116.82(17) . . ? C1 C6 C7 124.24(16) . . ? N1 C7 C6 124.64(17) . . ? N1 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? O2 C8 C13 106.90(15) . . ? O2 C8 C9 111.26(14) . . ? C13 C8 C9 104.40(15) . . ? O2 C8 H8 111.3 . . ? C13 C8 H8 111.3 . . ? C9 C8 H8 111.3 . . ? C10 C9 C14 101.84(15) . . ? C10 C9 C8 105.77(14) . . ? C14 C9 C8 100.28(14) . . ? C10 C9 Pd1 122.86(13) . . ? C14 C9 Pd1 119.02(12) . . ? C8 C9 Pd1 104.21(11) . . ? C9 C10 C11 104.27(15) . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10B 110.9 . . ? C11 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C12 C11 C10 102.44(15) . . ? C12 C11 H11A 111.3 . . ? C10 C11 H11A 111.3 . . ? C12 C11 H11B 111.3 . . ? C10 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? C11 C12 C13 108.04(17) . . ? C11 C12 C14 101.98(16) . . ? C13 C12 C14 101.46(16) . . ? C11 C12 H12 114.6 . . ? C13 C12 H12 114.6 . . ? C14 C12 H12 114.6 . . ? C8 C13 C12 103.13(15) . . ? C8 C13 H13A 111.1 . . ? C12 C13 H13A 111.1 . . ? C8 C13 H13B 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.1 . . ? C9 C14 C12 94.81(14) . . ? C9 C14 H14A 112.8 . . ? C12 C14 H14A 112.8 . . ? C9 C14 H14B 112.8 . . ? C12 C14 H14B 112.8 . . ? H14A C14 H14B 110.2 . . ? C20 C15 C16 119.27(17) . . ? C20 C15 P1 123.63(15) . . ? C16 C15 P1 117.05(14) . . ? C17 C16 C15 120.57(19) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.00(19) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 119.7(2) . . ? C15 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C26 C21 C22 119.32(16) . . ? C26 C21 P1 119.13(13) . . ? C22 C21 P1 121.45(13) . . ? C23 C22 C21 120.17(17) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.94(18) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.47(17) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.72(17) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.37(17) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C32 C27 C28 118.87(16) . . ? C32 C27 P1 116.00(13) . . ? C28 C27 P1 125.13(14) . . ? C29 C28 C27 119.96(17) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.33(17) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.08(18) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 119.77(18) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C27 120.99(17) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C7 N1 O2 114.50(14) . . ? C7 N1 Pd1 129.45(13) . . ? O2 N1 Pd1 115.92(10) . . ? C1 O1 Pd1 126.70(12) . . ? N1 O2 C8 106.50(13) . . ? N1 Pd1 C9 82.31(7) . . ? N1 Pd1 O1 88.86(6) . . ? C9 Pd1 O1 171.17(6) . . ? N1 Pd1 P1 178.82(4) . . ? C9 Pd1 P1 97.51(5) . . ? O1 Pd1 P1 91.31(4) . . ? C27 P1 C21 107.88(8) . . ? C27 P1 C15 103.40(8) . . ? C21 P1 C15 102.57(8) . . ? C27 P1 Pd1 116.39(6) . . ? C21 P1 Pd1 112.49(6) . . ? C15 P1 Pd1 112.86(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 177.13(18) . . . . ? C6 C1 C2 C3 -2.1(3) . . . . ? C1 C2 C3 C4 1.4(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 -1.2(3) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C4 C5 C6 C7 179.44(18) . . . . ? O1 C1 C6 C5 -178.00(18) . . . . ? C2 C1 C6 C5 1.1(3) . . . . ? O1 C1 C6 C7 3.1(3) . . . . ? C2 C1 C6 C7 -177.75(17) . . . . ? C5 C6 C7 N1 -174.45(17) . . . . ? C1 C6 C7 N1 4.4(3) . . . . ? O2 C8 C9 C10 174.83(14) . . . . ? C13 C8 C9 C10 -70.21(18) . . . . ? O2 C8 C9 C14 -79.63(17) . . . . ? C13 C8 C9 C14 35.33(18) . . . . ? O2 C8 C9 Pd1 44.05(16) . . . . ? C13 C8 C9 Pd1 159.01(12) . . . . ? C14 C9 C10 C11 -32.33(18) . . . . ? C8 C9 C10 C11 72.07(18) . . . . ? Pd1 C9 C10 C11 -168.84(12) . . . . ? C9 C10 C11 C12 -2.63(19) . . . . ? C10 C11 C12 C13 -69.68(19) . . . . ? C10 C11 C12 C14 36.74(19) . . . . ? O2 C8 C13 C12 117.55(16) . . . . ? C9 C8 C13 C12 -0.44(19) . . . . ? C11 C12 C13 C8 72.05(19) . . . . ? C14 C12 C13 C8 -34.73(19) . . . . ? C10 C9 C14 C12 53.46(17) . . . . ? C8 C9 C14 C12 -55.22(16) . . . . ? Pd1 C9 C14 C12 -167.92(13) . . . . ? C11 C12 C14 C9 -55.76(17) . . . . ? C13 C12 C14 C9 55.71(17) . . . . ? C20 C15 C16 C17 -0.8(3) . . . . ? P1 C15 C16 C17 -178.59(14) . . . . ? C15 C16 C17 C18 1.2(3) . . . . ? C16 C17 C18 C19 -0.7(3) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C16 C15 C20 C19 -0.1(3) . . . . ? P1 C15 C20 C19 177.54(15) . . . . ? C18 C19 C20 C15 0.6(3) . . . . ? C26 C21 C22 C23 0.8(3) . . . . ? P1 C21 C22 C23 177.13(14) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C22 C23 C24 C25 0.5(3) . . . . ? C23 C24 C25 C26 -0.3(3) . . . . ? C24 C25 C26 C21 0.3(3) . . . . ? C22 C21 C26 C25 -0.6(3) . . . . ? P1 C21 C26 C25 -176.99(14) . . . . ? C32 C27 C28 C29 0.1(3) . . . . ? P1 C27 C28 C29 -179.14(14) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C29 C30 C31 C32 0.0(3) . . . . ? C30 C31 C32 C27 0.0(3) . . . . ? C28 C27 C32 C31 0.0(3) . . . . ? P1 C27 C32 C31 179.24(15) . . . . ? C6 C7 N1 O2 179.04(15) . . . . ? C6 C7 N1 Pd1 -5.4(3) . . . . ? C2 C1 O1 Pd1 172.17(13) . . . . ? C6 C1 O1 Pd1 -8.7(3) . . . . ? C7 N1 O2 C8 -154.96(15) . . . . ? Pd1 N1 O2 C8 28.83(16) . . . . ? C13 C8 O2 N1 -161.23(14) . . . . ? C9 C8 O2 N1 -47.83(18) . . . . ? C32 C27 P1 C21 173.02(14) . . . . ? C28 C27 P1 C21 -7.77(18) . . . . ? C32 C27 P1 C15 -78.81(15) . . . . ? C28 C27 P1 C15 100.40(16) . . . . ? C32 C27 P1 Pd1 45.52(15) . . . . ? C28 C27 P1 Pd1 -135.27(14) . . . . ? C26 C21 P1 C27 -119.04(14) . . . . ? C22 C21 P1 C27 64.64(16) . . . . ? C26 C21 P1 C15 132.22(14) . . . . ? C22 C21 P1 C15 -44.11(16) . . . . ? C26 C21 P1 Pd1 10.68(15) . . . . ? C22 C21 P1 Pd1 -165.64(13) . . . . ? C20 C15 P1 C27 13.81(17) . . . . ? C16 C15 P1 C27 -168.55(14) . . . . ? C20 C15 P1 C21 125.92(16) . . . . ? C16 C15 P1 C21 -56.44(15) . . . . ? C20 C15 P1 Pd1 -112.79(15) . . . . ? C16 C15 P1 Pd1 64.85(14) . . . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.059 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL rz1742 in P-1 CELL 1.54184 9.1130 11.3390 13.8100 109.376 105.198 93.408 ZERR 2.00 0.0009 0.0011 0.0012 0.003 0.004 0.003 LATT 1 SFAC C H N O PD P UNIT 64 60 2 4 2 2 MERG 2 FMAP 2 PLAN 10 size .19 .10 .067 omit -2 -13 8 omit -6 -11 9 omit -3 -13 10 omit -5 -12 10 omit -6 -11 11 ACTA BOND $H CONF LIST 4 L.S. 8 TEMP -173.00 WGHT 0.026400 1.003500 FVAR 4.99501 C1 1 0.107685 0.247473 0.087954 11.00000 0.02082 0.02666 = 0.02149 0.00909 0.00650 0.00706 C2 1 -0.047304 0.184723 0.050030 11.00000 0.02522 0.02986 = 0.02678 0.01071 0.00831 0.00430 AFIX 43 H2 2 -0.075342 0.124660 0.078980 11.00000 -1.20000 AFIX 0 C3 1 -0.157459 0.208565 -0.027238 11.00000 0.02055 0.03439 = 0.02334 0.00511 0.00459 0.00431 AFIX 43 H3 2 -0.260427 0.166245 -0.049538 11.00000 -1.20000 AFIX 0 C4 1 -0.120784 0.293620 -0.073375 11.00000 0.02581 0.04036 = 0.02301 0.01225 0.00153 0.00831 AFIX 43 H4 2 -0.197790 0.309953 -0.126608 11.00000 -1.20000 AFIX 0 C5 1 0.028209 0.353552 -0.040868 11.00000 0.03150 0.03410 = 0.02433 0.01492 0.00790 0.00980 AFIX 43 H5 2 0.053666 0.410462 -0.073460 11.00000 -1.20000 AFIX 0 C6 1 0.145472 0.333618 0.039565 11.00000 0.02458 0.02389 = 0.01872 0.00708 0.00772 0.00831 C7 1 0.297252 0.401272 0.065685 11.00000 0.02878 0.02077 = 0.01902 0.00973 0.00963 0.00788 AFIX 43 H7 2 0.308992 0.461104 0.032634 11.00000 -1.20000 AFIX 0 C8 1 0.680956 0.396970 0.175156 11.00000 0.02413 0.02539 = 0.02582 0.01208 0.01042 0.00459 AFIX 13 H8 2 0.688667 0.323704 0.112839 11.00000 -1.20000 AFIX 0 C9 1 0.665562 0.354945 0.268321 11.00000 0.01841 0.02096 = 0.02053 0.00819 0.00580 0.00106 C10 1 0.794852 0.277756 0.287329 11.00000 0.02222 0.02911 = 0.02739 0.01339 0.00908 0.00427 AFIX 23 H10A 2 0.798336 0.214988 0.218529 11.00000 -1.20000 H10B 2 0.780756 0.232743 0.335427 11.00000 -1.20000 AFIX 0 C11 1 0.944998 0.378691 0.341371 11.00000 0.02142 0.03805 = 0.03003 0.01550 0.00659 0.00215 AFIX 23 H11A 2 0.996202 0.382900 0.415403 11.00000 -1.20000 H11B 2 1.018454 0.360057 0.298749 11.00000 -1.20000 AFIX 0 C12 1 0.883686 0.501066 0.341721 11.00000 0.02566 0.02889 = 0.02779 0.00842 0.00760 -0.00312 AFIX 13 H12 2 0.955051 0.580222 0.393386 11.00000 -1.20000 AFIX 0 C13 1 0.829013 0.495306 0.224639 11.00000 0.02615 0.02976 = 0.03190 0.01427 0.00984 0.00057 AFIX 23 H13A 2 0.807391 0.578744 0.221573 11.00000 -1.20000 H13B 2 0.906813 0.467514 0.187192 11.00000 -1.20000 AFIX 0 C14 1 0.728780 0.481075 0.364373 11.00000 0.02636 0.02561 = 0.02411 0.00610 0.00827 0.00007 AFIX 23 H14A 2 0.741460 0.471352 0.434611 11.00000 -1.20000 H14B 2 0.666428 0.548368 0.358505 11.00000 -1.20000 AFIX 0 C15 1 0.279190 0.112505 0.345450 11.00000 0.02022 0.02052 = 0.02731 0.01371 0.01171 0.00884 C16 1 0.162866 0.033634 0.254182 11.00000 0.02267 0.02433 = 0.03092 0.01315 0.00994 0.00561 AFIX 43 H16 2 0.181720 0.005639 0.186304 11.00000 -1.20000 AFIX 0 C17 1 0.020352 -0.004086 0.261791 11.00000 0.02046 0.03038 = 0.04593 0.02131 0.00874 0.00568 AFIX 43 H17 2 -0.057385 -0.059054 0.199504 11.00000 -1.20000 AFIX 0 C18 1 -0.008977 0.038009 0.359670 11.00000 0.02517 0.03834 = 0.06068 0.03207 0.02485 0.01439 AFIX 43 H18 2 -0.107204 0.012749 0.364612 11.00000 -1.20000 AFIX 0 C19 1 0.104751 0.117075 0.450708 11.00000 0.04007 0.04050 = 0.04768 0.02644 0.03188 0.01908 AFIX 43 H19 2 0.084137 0.146183 0.517971 11.00000 -1.20000 AFIX 0 C20 1 0.249799 0.154304 0.444153 11.00000 0.02951 0.02758 = 0.03052 0.01490 0.01593 0.01020 AFIX 43 H20 2 0.327908 0.207926 0.506878 11.00000 -1.20000 AFIX 0 C21 1 0.516757 0.008113 0.262650 11.00000 0.01572 0.01727 = 0.01955 0.00503 0.00560 0.00335 C22 1 0.504534 -0.091259 0.299993 11.00000 0.02323 0.02089 = 0.02298 0.00867 0.00942 0.00455 AFIX 43 H22 2 0.471130 -0.079172 0.361756 11.00000 -1.20000 AFIX 0 C23 1 0.541029 -0.207587 0.247162 11.00000 0.02647 0.02020 = 0.03122 0.01029 0.00998 0.00567 AFIX 43 H23 2 0.533864 -0.274753 0.273245 11.00000 -1.20000 AFIX 0 C24 1 0.587991 -0.225770 0.156219 11.00000 0.02640 0.01930 = 0.02889 0.00348 0.00985 0.00776 AFIX 43 H24 2 0.612088 -0.305762 0.119839 11.00000 -1.20000 AFIX 0 C25 1 0.599995 -0.128234 0.118100 11.00000 0.02324 0.02306 = 0.02388 0.00441 0.01058 0.00430 AFIX 43 H25 2 0.632677 -0.141062 0.055965 11.00000 -1.20000 AFIX 0 C26 1 0.564041 -0.011415 0.171090 11.00000 0.01882 0.01935 = 0.02081 0.00706 0.00675 0.00277 AFIX 43 H26 2 0.571719 0.055507 0.144791 11.00000 -1.20000 AFIX 0 C27 1 0.590923 0.230891 0.462349 11.00000 0.01977 0.02017 = 0.01864 0.00755 0.00856 0.00393 C28 1 0.699023 0.171067 0.512605 11.00000 0.02093 0.02178 = 0.02378 0.01106 0.00920 0.00567 AFIX 43 H28 2 0.710048 0.086866 0.474782 11.00000 -1.20000 AFIX 0 C29 1 0.790645 0.234754 0.618108 11.00000 0.02109 0.03361 = 0.02525 0.01626 0.00611 0.00476 AFIX 43 H29 2 0.864150 0.193826 0.652215 11.00000 -1.20000 AFIX 0 C30 1 0.775257 0.357661 0.673757 11.00000 0.02598 0.03312 = 0.01808 0.00879 0.00575 -0.00378 AFIX 43 H30 2 0.838167 0.400703 0.745816 11.00000 -1.20000 AFIX 0 C31 1 0.668830 0.417475 0.624684 11.00000 0.03502 0.02316 = 0.02227 0.00469 0.01276 0.00366 AFIX 43 H31 2 0.658274 0.501720 0.662773 11.00000 -1.20000 AFIX 0 C32 1 0.577193 0.354286 0.519520 11.00000 0.02851 0.02247 = 0.02142 0.00953 0.00847 0.00855 AFIX 43 H32 2 0.503932 0.395859 0.485993 11.00000 -1.20000 AFIX 0 N1 3 0.418392 0.386642 0.130617 11.00000 0.02204 0.01913 = 0.02029 0.00891 0.00820 0.00320 O1 4 0.202172 0.222800 0.164353 11.00000 0.01870 0.03707 = 0.03319 0.02253 0.00377 0.00196 O2 4 0.555245 0.462099 0.142439 11.00000 0.02341 0.02452 = 0.03018 0.01547 0.00755 0.00174 PD1 5 0.438057 0.281040 0.224038 11.00000 0.01736 0.01598 = 0.01631 0.00688 0.00606 0.00389 P1 6 0.461510 0.159724 0.326032 11.00000 0.01755 0.01602 = 0.01719 0.00686 0.00757 0.00498 HKLF 4 REM rz1742 in P-1 REM R1 = 0.0207 for 5220 Fo > 4sig(Fo) and 0.0210 for all 5283 data REM 334 parameters refined using 0 restraints END WGHT 0.0274 0.9666 REM Highest difference peak 0.410, deepest hole -0.498, 1-sigma level 0.059 Q1 1 0.4614 0.2133 0.2864 11.00000 0.05 0.41 Q2 1 0.5898 0.3278 0.2455 11.00000 0.05 0.39 Q3 1 0.5472 0.1989 0.4116 11.00000 0.05 0.34 Q4 1 0.6565 0.5012 0.2614 11.00000 0.05 0.33 Q5 1 0.3802 0.3431 0.2780 11.00000 0.05 0.32 Q6 1 0.3648 0.1398 0.3440 11.00000 0.05 0.32 Q7 1 0.5887 -0.0687 0.1439 11.00000 0.05 0.31 Q8 1 0.5438 0.0003 0.2205 11.00000 0.05 0.31 Q9 1 0.4051 0.3458 0.1539 11.00000 0.05 0.30 Q10 1 0.1388 0.3124 0.0816 11.00000 0.05 0.30 ; _shelx_res_checksum 7594 _shelx_hkl_file ; 0 0 -1 1172.73 58.1903 1 0 0 1 1261.36 57.3482 22 0 0 1 1147.42 58.3460 20 0 0 -1 1254.61 66.0010 21 0 0 2 370193. 3414.62 22 0 0 -2 345893. 3436.35 1 0 0 2 361226. 3449.90 20 0 0 -2 350761. 3477.23 21 0 0 -3 931.569 99.2772 1 0 0 3 925.354 99.1221 20 0 0 -3 860.997 100.853 21 0 0 3 876.720 86.8197 22 0 0 4 38615.0 746.595 20 0 0 -4 38421.3 742.598 1 0 0 -4 41821.1 792.687 21 0 0 4 40582.1 733.844 22 0 0 5 1652.52 155.880 22 0 0 -5 1413.27 151.153 1 0 0 -5 1526.95 161.129 21 0 0 5 1814.44 178.508 20 0 0 -6 619.466 119.387 21 0 0 6 632.162 115.666 22 0 0 -6 469.453 101.695 1 0 0 6 708.980 128.843 20 0 0 -7 108474. 1803.69 21 0 0 -7 108550. 1800.50 1 0 0 7 107516. 1758.84 22 0 0 7 107842. 1835.19 20 0 0 -8 3510.00 309.856 21 0 0 8 4341.31 352.749 20 0 0 -8 4666.64 347.638 1 0 0 8 4278.95 325.891 22 0 0 9 41450.6 1123.96 22 0 0 9 40494.4 1202.30 20 0 0 -9 40298.7 1149.65 21 0 0 -9 40807.9 1150.06 1 0 0 -10 27264.3 990.416 21 0 0 -10 29235.9 626.564 12 0 0 -10 30006.0 1018.48 1 0 0 -10 29693.5 600.927 6 0 0 10 29065.7 605.994 15 0 0 10 30005.5 1083.06 20 0 0 -11 46921.6 847.205 12 0 0 11 47051.0 821.871 15 0 0 -11 45761.2 807.203 6 0 0 -12 746.462 100.600 12 0 0 -12 779.902 96.8743 6 0 0 12 802.017 95.8718 15 0 0 13 16827.0 420.967 15 0 0 -13 16655.3 434.146 12 0 0 14 1736.09 116.392 15 0 0 15 3787.24 136.737 15 0 1 -16 68.7975 19.3405 14 0 -1 15 10427.7 251.469 15 0 1 -15 9952.71 219.958 18 0 -1 14 297.877 58.3815 15 0 -1 13 16491.0 425.738 15 0 1 -13 16726.9 447.941 12 0 -1 12 6002.38 258.739 15 0 1 -12 5783.35 257.238 6 0 1 -12 6378.89 281.187 12 0 1 -11 1138.51 210.604 21 0 1 -11 1117.71 193.945 1 0 1 -11 1114.74 124.804 12 0 -1 11 967.830 199.955 20 0 -1 11 1167.56 115.653 15 0 1 -11 1164.05 118.369 6 0 1 -10 62395.2 1491.01 21 0 -1 10 66951.6 1004.80 15 0 1 -10 68068.6 1045.31 12 0 1 -10 66717.0 993.840 6 0 -1 10 66539.2 1628.61 20 0 1 -10 66530.5 1523.52 1 0 -1 9 2405.71 246.365 22 0 1 -9 2862.89 279.828 1 0 -1 9 2495.05 280.337 20 0 1 -9 2408.37 254.941 21 0 -1 8 124494. 2077.90 20 0 1 -8 120308. 1960.33 1 0 -1 8 120619. 1913.36 22 0 1 -8 116353. 1949.83 21 0 -1 7 25234.3 764.124 20 0 -1 7 26946.1 719.923 22 0 1 -7 24652.9 708.875 21 0 1 -7 26162.2 741.383 1 0 1 -6 23886.2 642.931 21 0 1 -6 24323.2 650.696 1 0 -1 6 23101.9 669.079 20 0 -1 6 24592.9 627.846 22 0 1 -5 7079.52 305.052 1 0 -1 5 7558.21 333.296 20 0 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57526.9 819.195 2 0 2 -4 57899.8 826.977 21 0 -2 4 60652.1 943.926 20 0 2 -4 58075.1 846.105 1 0 2 -3 189535. 1979.58 4 0 -2 3 192896. 2108.24 20 0 2 -3 190341. 1972.09 1 0 2 -3 186172. 1952.41 21 0 -2 2 175496. 1739.18 23 0 2 -2 156615. 1836.42 2 0 2 -2 168820. 1720.80 5 0 2 -2 159820. 1691.09 4 0 -2 1 140858. 1526.99 23 0 -2 1 139759. 1343.25 21 0 2 -1 136122. 1610.53 2 0 2 -1 136222. 1471.76 4 0 -2 1 141242. 1374.68 1 0 2 -1 138324. 1440.30 5 0 -2 0 215011. 2155.35 1 0 2 0 213202. 2326.92 2 0 2 0 219605. 2234.20 22 0 2 1 380.269 67.7810 2 0 2 1 298.825 59.6085 20 0 2 1 339.526 65.9671 22 0 -2 -1 225.778 57.1912 1 0 2 2 165647. 1833.86 2 0 -2 -2 167777. 1951.65 1 0 2 2 167668. 1952.10 20 0 -2 -2 170148. 2024.99 21 0 2 3 59.9453 56.8560 20 0 -2 -3 189.706 69.0548 21 0 2 3 67.9354 57.7878 22 0 -2 -3 132.475 65.9010 1 0 2 3 128.653 33.2630 2 0 2 4 180880. 2315.11 20 0 -2 -4 177858. 2310.87 1 0 -2 -4 184840. 2390.06 21 0 2 4 177830. 2313.86 22 0 2 5 2117.63 213.822 20 0 -2 -5 2023.54 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4845.64 221.893 6 0 -4 11 5201.32 221.872 15 0 4 -11 5155.45 416.709 5 0 -4 11 5007.62 429.676 20 0 4 -10 9641.35 335.691 12 0 -4 10 9176.55 565.099 20 0 4 -10 10434.6 569.127 5 0 -4 9 34135.5 1053.38 20 0 4 -9 33727.9 987.573 5 0 4 -8 1082.62 163.566 5 0 -4 8 813.944 150.447 20 0 4 -7 205339. 2652.61 5 0 -4 7 195450. 2710.79 20 0 -4 6 1830.56 142.631 23 0 4 -6 2209.26 183.940 2 0 4 -6 2059.60 182.328 5 0 -4 6 1824.90 189.991 20 0 4 -6 2156.18 148.316 1 0 -4 5 389975. 3968.80 23 0 4 -5 384288. 3799.10 1 0 4 -5 380533. 3924.95 4 0 4 -5 377904. 4045.31 5 0 -4 5 382101. 4164.81 20 0 4 -4 2652.46 160.021 4 0 4 -4 2643.52 125.046 1 0 -4 4 2499.58 167.470 23 0 4 -4 2744.52 174.246 5 0 4 -4 2907.33 225.926 2 0 4 -3 346793. 3499.21 4 0 4 -3 327352. 3470.84 5 0 -4 3 356924. 3584.69 23 0 4 -3 337225. 3796.85 2 0 4 -2 256797. 2788.93 4 0 -4 2 238476. 2400.53 3 0 -4 2 247454. 2478.92 21 0 -4 2 258630. 2856.45 23 0 4 -2 270158. 2755.46 5 0 4 -2 265159. 3068.94 2 0 -4 1 101068. 1218.16 1 0 4 -1 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417.904 20 1 -4 -8 4618.97 225.205 12 1 -4 -8 4368.26 418.750 1 1 -4 -8 4252.91 399.614 21 -1 4 8 4128.45 387.124 22 -1 4 8 4810.70 235.342 15 -1 4 7 48796.8 1350.83 22 1 -4 -7 50049.0 1365.59 21 -1 4 7 50927.6 1422.74 20 1 -4 -7 54105.8 1436.81 1 1 -4 -7 52789.7 848.550 12 1 -4 -6 134144. 2269.90 21 1 -4 -6 132668. 2294.58 1 -1 4 6 123888. 2234.65 22 -1 4 6 127179. 2296.56 20 1 -4 -5 28756.6 888.118 1 -1 4 5 27191.5 887.083 20 -1 4 5 26508.0 863.825 22 1 -4 -5 25773.4 829.570 21 1 -4 -5 26803.4 741.873 23 1 -4 -4 119669. 1905.93 21 1 -4 -4 118771. 1807.41 23 1 -4 -4 123796. 1944.46 1 -1 4 4 117383. 1649.86 2 -1 4 4 125152. 1977.52 20 -1 4 4 119669. 1945.64 22 1 -4 -3 21468.6 652.991 1 -1 4 3 21642.3 661.379 20 1 -4 -3 20901.2 633.130 21 1 -4 -3 19989.0 621.321 23 -1 4 3 21850.5 678.589 22 -1 4 3 20670.1 592.924 2 -1 4 2 205498. 2087.07 19 -1 4 2 211606. 2608.83 22 1 -4 -2 205841. 2588.82 23 1 -4 -2 209640. 2501.43 21 1 -4 -2 214214. 2564.83 1 -1 4 2 209928. 2616.74 2 -1 4 1 4899.85 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65396.1 1472.20 1 -3 5 4 64282.1 1388.01 2 3 -5 -3 6342.63 402.721 23 3 -5 -3 6506.61 395.399 3 3 -5 -3 6399.66 402.814 1 -3 5 3 6562.77 414.268 2 3 -5 -2 24616.5 806.859 23 3 -5 -2 26160.8 752.010 3 -3 5 2 25902.0 649.851 19 -3 5 2 26735.9 872.124 2 3 -5 -2 26579.9 789.109 1 3 -5 -1 35579.6 973.830 23 3 -5 -1 35832.8 852.659 3 -3 5 1 34268.1 774.582 19 -3 5 1 34745.9 1011.03 2 3 -5 0 72776.8 1482.69 23 -3 5 0 72708.7 1255.85 19 3 -5 0 77350.7 1294.34 3 -3 5 0 76942.1 1578.08 2 3 -5 1 31156.9 893.943 23 3 -5 1 30109.6 719.934 3 -3 5 -1 28586.1 746.983 19 -3 5 -1 29366.2 921.165 2 -3 5 -2 45021.5 1025.56 19 3 -5 2 47226.8 1124.26 23 3 -5 2 48208.3 923.537 3 -3 5 -2 49044.9 1208.27 2 3 -5 3 16176.4 612.633 23 3 -5 3 15447.9 507.197 20 -3 5 -3 15933.4 608.285 19 3 -5 3 14924.7 494.062 3 -3 5 -3 15312.1 640.560 2 3 -5 4 26523.9 710.609 20 -3 5 -4 25680.2 850.903 19 3 -5 4 26766.4 815.246 23 3 -5 4 25704.4 678.829 3 -3 5 -4 25742.6 844.206 2 3 -5 5 144757. 2091.10 20 -3 5 -5 140326. 2399.54 19 -3 5 -5 138125. 2130.00 1 3 -5 5 137464. 2215.41 23 -3 5 -6 47.1973 46.3882 1 3 -5 6 113.412 69.5861 23 3 -5 6 25.5007 55.7051 20 3 -5 7 34607.0 987.136 20 3 -5 7 33293.4 984.772 23 -3 5 -7 34354.0 1016.42 1 3 -5 8 12324.4 361.408 15 -3 5 -8 13128.1 641.936 1 3 -5 9 9143.93 581.154 22 3 -5 9 9217.71 316.735 15 3 -5 10 16451.7 439.234 15 3 -5 10 17490.0 496.084 24 3 -5 11 3748.25 212.536 24 3 -5 11 3474.73 192.946 15 3 -5 12 52734.7 845.198 24 3 -5 12 47871.4 774.344 15 3 -5 13 10277.6 287.678 24 3 -5 13 10353.5 279.213 15 -3 5 -14 61377.2 758.785 13 3 -5 14 59012.4 714.528 15 3 -4 -14 11767.9 224.893 12 -3 4 14 11737.4 217.088 15 -3 4 13 2809.85 133.734 17 -3 4 13 2842.40 131.531 15 3 -4 -13 2868.40 138.038 12 -3 4 12 20010.5 441.408 17 -3 4 12 19429.0 433.290 15 3 -4 -11 1689.13 138.127 12 -3 4 11 1998.57 149.423 15 3 -4 -10 34039.8 680.271 12 3 -4 -10 33636.4 694.912 16 -3 4 10 35362.2 703.974 15 3 -4 -9 14834.3 430.181 12 3 -4 -9 15401.4 447.486 16 -3 4 9 15829.0 454.875 15 3 -4 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24233.9 689.537 19 3 -4 2 24040.4 612.545 3 3 -4 2 23789.7 703.528 23 3 -4 3 46944.6 870.409 20 3 -4 3 46771.3 925.548 3 -3 4 -3 49427.8 1085.44 19 3 -4 3 48361.2 1056.89 23 -3 4 -3 48008.2 1094.38 2 3 -4 4 9837.86 390.137 20 3 -4 4 9913.83 459.157 23 -3 4 -4 9940.30 497.039 19 -3 4 -4 9805.05 466.442 2 3 -4 4 9968.01 408.859 3 -3 4 -5 129903. 2045.50 1 -3 4 -5 135944. 2288.87 19 3 -4 5 130864. 1929.41 20 3 -4 5 135990. 2089.41 23 -3 4 -5 136583. 2067.47 2 3 -4 6 141225. 2172.06 23 -3 4 -6 133639. 2416.35 19 3 -4 6 139510. 2097.27 20 -3 4 -6 136710. 2210.07 1 3 -4 7 32542.5 925.409 20 3 -4 7 34489.5 956.180 23 -3 4 -7 33319.3 1013.82 1 3 -4 8 20798.0 485.343 15 -3 4 -8 19307.6 796.612 1 3 -4 8 20265.9 848.384 22 -3 4 -9 17224.2 775.362 1 3 -4 9 16537.3 441.103 15 3 -4 9 15467.6 752.842 22 3 -4 10 36674.7 743.444 24 3 -4 10 35288.7 691.442 15 3 -4 11 20778.9 516.963 24 3 -4 11 20696.7 495.414 15 3 -4 12 1044.57 105.965 24 3 -4 12 875.317 95.8090 15 3 -4 13 30043.8 520.492 24 3 -4 13 32578.4 553.233 15 -3 4 -14 4237.64 153.320 13 3 -4 14 4476.58 152.775 15 3 -3 -14 17008.7 331.258 12 -3 3 14 16910.9 318.165 15 3 -3 -13 29553.9 549.696 12 -3 3 13 30564.5 540.893 17 -3 3 13 29771.1 539.545 15 3 -3 -12 185.914 60.0762 12 -3 3 12 117.675 53.9782 15 3 -3 -11 39382.0 742.057 12 -3 3 11 39911.5 752.240 15 3 -3 -10-21.7993 44.2862 12 3 -3 -10 22.8468 47.7891 16 -3 3 10-33.4344 55.2765 15 3 -3 -9 1403.76 126.648 12 -3 3 9 1137.86 198.776 20 3 -3 -9 1597.89 142.249 16 3 -3 -9 1621.41 261.818 1 -3 3 9 1519.33 134.043 15 3 -3 -8 15792.6 419.098 12 -3 3 8 14796.5 707.977 20 3 -3 -8 15668.5 426.042 16 3 -3 -8 15328.5 744.273 1 -3 3 8 15298.6 427.873 15 3 -3 -8 14307.1 741.936 21 3 -3 -7 20595.4 840.298 21 -3 3 7 21170.1 795.501 20 -3 3 7 21068.4 710.441 19 3 -3 -7 21121.7 827.696 1 3 -3 -6 53486.7 1307.22 21 -3 3 6 56146.5 1255.07 20 3 -3 -6 55288.6 1313.15 1 -3 3 6 55853.1 1163.44 19 3 -3 -5 392.884 112.300 1 3 -3 -5 504.962 117.460 21 -3 3 5 741.150 129.303 20 -3 3 5 582.953 110.530 19 -3 3 4 176045. 2224.54 20 3 -3 -4 169189. 2184.73 23 -3 3 4 158074. 2120.10 19 3 -3 -4 164085. 2320.94 1 3 -3 -3 61190.1 1122.28 23 3 -3 -3 62237.9 1165.28 3 3 -3 -3 62141.1 1166.70 1 -3 3 3 60479.6 1059.89 19 3 -3 -2 175766. 2215.09 3 3 -3 -2 174062. 2265.22 23 -3 3 2 170393. 2127.85 19 3 -3 -2 172288. 2219.69 1 3 -3 -1 2546.66 207.958 23 -3 3 1 2818.34 195.323 19 3 -3 -1 3108.47 205.355 3 3 -3 0 60206.5 1111.14 23 3 -3 0 59189.4 1007.73 3 -3 3 0 58169.6 1016.29 19 3 -3 1 7351.69 313.708 3 -3 3 -1 7203.27 326.669 19 3 -3 1 7359.89 352.537 23 -3 3 -2 9321.13 268.796 21 3 -3 2 9901.31 419.874 23 3 -3 2 8842.68 284.447 20 -3 3 -2 9659.82 405.446 19 3 -3 2 9396.67 364.294 3 -3 3 -3 3777.01 188.894 21 3 -3 3 4546.93 289.343 23 3 -3 3 4428.87 222.602 20 3 -3 3 4308.31 257.958 3 -3 3 -3 4243.45 287.984 19 -3 3 -4 19108.7 495.324 21 3 -3 4 18454.7 632.329 23 -3 3 -4 19605.7 631.966 1 -3 3 -4 19130.1 676.795 19 3 -3 4 20583.2 611.087 3 3 -3 4 19254.6 535.619 20 3 -3 5 139881. 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3 -2 -11 9246.63 303.497 6 3 -2 -11 9285.17 353.184 16 3 -2 -10 41796.5 769.313 12 -3 2 10 39499.9 1263.68 20 3 -2 -10 42221.7 728.906 6 3 -2 -10 40774.6 794.846 16 3 -2 -10 42511.4 1321.70 1 -3 2 10 41160.0 776.163 15 3 -2 -9-6.28913 45.4119 12 -3 2 9 43.7443 61.3999 20 -3 2 9-2.74889 58.6280 19 3 -2 -9 101.834 45.3978 6 3 -2 -9 101.473 41.6879 16 -3 2 9 168.872 53.8704 15 -3 2 8 26525.2 861.322 19 -3 2 8 25888.6 902.480 20 3 -2 -8 28078.5 965.660 1 3 -2 -7 2639.96 289.720 21 -3 2 7 2185.32 233.477 20 -3 2 7 2466.42 239.483 19 3 -2 -7 2426.44 261.463 1 -3 2 6 74329.9 1368.48 19 3 -2 -6 70148.1 1478.67 21 -3 2 6 74024.0 1373.05 20 3 -2 -6 70247.8 1429.43 1 -3 2 5 56761.6 1083.21 20 -3 2 5 55084.8 1085.38 19 3 -2 -5 54604.4 1150.61 1 -3 2 4 1029.46 120.674 20 -3 2 4 1138.02 134.806 19 3 -2 -4 901.346 102.872 23 3 -2 -4 1072.24 145.262 1 3 -2 -3 109911. 1510.06 23 3 -2 -3 115199. 1623.39 3 -3 2 3 108434. 1422.49 20 -3 2 3 112080. 1550.67 19 3 -2 -3 112841. 1603.93 1 3 -2 -2 14273.0 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1014.95 22 3 -2 7 32681.5 925.850 20 -3 2 -7 33653.9 1053.24 1 -3 2 -8 41929.1 1252.58 1 3 -2 8 41626.7 1256.45 22 3 -2 8 43989.1 725.144 10 3 -2 8 43836.0 766.804 15 3 -2 9 304.228 70.3374 24 3 -2 9 215.328 111.332 22 3 -2 9 350.574 61.8161 10 -3 2 -9 291.467 118.941 1 3 -2 9 302.632 70.5545 15 3 -2 10 58492.0 940.334 24 3 -2 10 58999.7 881.384 10 3 -2 10 57898.0 952.728 15 3 -2 11 7069.52 242.429 10 3 -2 11 6885.95 278.973 15 3 -2 12 7320.63 265.268 15 3 -2 13 7035.63 227.625 15 3 -2 14 9085.51 213.516 15 3 -1 -15 7177.48 211.302 12 -3 1 15 7231.23 197.836 15 3 -1 -14 13938.9 360.340 12 3 -1 -14 14129.0 333.787 6 -3 1 14 13632.0 341.498 15 3 -1 -13 24435.7 500.531 6 3 -1 -13 23356.3 532.484 12 -3 1 13 23372.9 515.933 15 3 -1 -12 25736.8 589.516 12 3 -1 -12 27238.9 563.404 6 -3 1 12 26058.4 578.976 15 3 -1 -11 99923.3 1370.49 12 3 -1 -11 97371.2 1315.02 6 -3 1 11 100799. 1368.98 15 3 -1 -10 41310.4 754.403 12 -3 1 10 39768.7 1230.86 20 3 -1 -10 41555.6 735.279 6 3 -1 -10 41882.8 1251.00 1 3 -1 -10 41266.8 782.717 16 -3 1 10 42037.2 767.804 15 -3 1 9 72404.8 1627.02 20 3 -1 -9 75283.6 1662.24 1 -3 1 8 3370.88 301.520 20 3 -1 -8 3611.65 317.008 1 -3 1 7 30675.8 865.790 20 3 -1 -7 30333.9 878.888 1 -3 1 6 18204.1 596.992 20 3 -1 -6 18974.1 632.077 1 -3 1 5 19365.0 551.534 20 3 -1 -5 18887.5 582.579 1 -3 1 4 49564.4 946.581 19 3 -1 -4 50118.8 944.588 1 3 -1 -4 50848.7 971.341 3 -3 1 4 52674.8 868.271 20 3 -1 -4 50596.6 783.789 23 -3 1 3 88446.1 1293.83 19 3 -1 -3 85130.8 1179.11 23 -3 1 3 88205.7 1086.23 20 3 -1 -3 85044.8 1288.32 3 3 -1 -3 87170.1 1266.43 1 3 -1 -3 86266.0 1109.80 5 3 -1 -2 188800. 2122.56 3 3 -1 -2 185578. 2089.34 23 -3 1 2 184349. 2095.71 19 3 -1 -2 189239. 1809.83 5 -3 1 1 22205.9 517.483 19 3 -1 -1 23948.4 533.056 3 3 -1 -1 22880.7 542.214 23 -3 1 0 141193. 1780.90 19 3 -1 0 143092. 1854.22 23 -3 1 -1 4416.82 211.182 21 3 -1 1 4335.60 112.593 20 -3 1 -1 4553.28 242.513 19 3 -1 1 4583.38 261.155 23 3 -1 1 4475.07 244.919 3 -3 1 -2 120008. 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4 -3 -2 101586. 1619.82 3 4 -3 -2 100415. 1659.26 23 4 -3 -1 4406.39 306.357 23 -4 3 1 4271.95 280.632 19 4 -3 -1 4443.14 285.231 3 4 -3 0 37771.6 954.632 23 4 -3 0 38199.7 881.280 3 -4 3 0 38118.8 889.772 19 -4 3 -1 96172.8 1307.20 21 -4 3 -1 94213.8 1594.12 19 4 -3 1 97681.2 1701.20 23 4 -3 2 41536.7 1037.66 23 -4 3 -2 43622.6 787.141 21 -4 3 -2 42359.7 1017.13 19 4 -3 2 43419.7 981.829 3 -4 3 -3 60412.1 1298.52 19 4 -3 3 59172.2 1216.39 3 -4 3 -4 2309.98 255.993 19 -4 3 -4 2527.92 257.331 1 4 -3 4 2043.74 246.223 23 4 -3 4 2428.05 241.901 3 -4 3 -5 93261.4 1821.20 1 -4 3 -5 92873.8 1907.05 19 4 -3 5 91385.4 1758.44 23 4 -3 6 254.792 101.484 22 -4 3 -6 343.942 126.213 1 -4 3 -6 489.768 152.625 19 4 -3 7 97068.6 1328.23 15 4 -3 7 95970.5 1265.70 10 -4 3 -7 95803.4 2022.81 1 4 -3 7 96557.1 2087.89 22 4 -3 8 23894.2 583.157 24 4 -3 8 22460.2 495.469 10 4 -3 8 21962.9 947.101 22 4 -3 8 22297.1 536.681 15 -4 3 -8 22620.9 942.558 1 4 -3 9 68816.8 1080.10 24 4 -3 9 67496.5 979.159 10 4 -3 9 65832.6 1048.58 15 4 -3 10 3531.45 193.366 24 4 -3 10 3504.62 172.808 10 4 -3 10 3220.00 192.964 15 -4 3 -11 10378.2 289.977 7 4 -3 11 9638.32 291.488 24 4 -3 11 10366.4 326.576 15 -4 3 -12 10252.9 248.364 7 4 -3 12 10036.2 287.817 15 -4 3 -13 1318.72 76.8996 13 4 -3 13 1413.59 89.6669 15 4 -2 -15 2347.78 101.361 12 -4 2 15 2412.96 97.6186 15 4 -2 -14 46915.9 699.912 12 4 -2 -14 47678.0 629.544 6 -4 2 14 47684.6 686.584 15 4 -2 -13 3725.67 188.448 12 4 -2 -13 3855.70 165.550 6 -4 2 13 3601.49 181.791 15 4 -2 -12 81494.5 1088.31 6 4 -2 -12 81811.5 1163.84 12 4 -2 -12 78897.8 1188.50 16 -4 2 12 78872.2 1147.75 15 4 -2 -11 15400.2 435.206 12 4 -2 -11 16288.1 414.000 6 4 -2 -11 15147.2 453.603 16 -4 2 11 15159.9 435.448 15 4 -2 -10 14532.7 417.666 12 4 -2 -10 14658.3 399.570 6 4 -2 -10 14269.7 432.005 16 -4 2 10 14148.6 422.726 15 4 -2 -9 2076.13 149.702 12 4 -2 -9 1844.16 265.145 1 -4 2 9 1962.92 252.737 19 4 -2 -9 2133.19 289.850 3 -4 2 9 1765.20 244.649 20 4 -2 -9 1971.06 140.937 6 4 -2 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25561.4 857.943 3 4 -1 -7 25240.1 826.236 1 -4 1 7 24839.9 746.234 20 -4 1 7 24348.5 822.940 19 4 -1 -7 25434.5 800.235 5 4 -1 -6 7857.47 437.609 3 -4 1 6 8059.14 368.612 20 -4 1 6 8803.31 453.574 19 4 -1 -6 7296.62 408.519 1 4 -1 -6 7570.19 379.322 5 -4 1 5 15055.6 450.412 20 4 -1 -5 16537.0 587.385 3 -4 1 5 14796.5 556.218 19 4 -1 -5 16390.2 498.606 5 4 -1 -4 65775.5 1074.88 23 -4 1 4 63413.5 1201.57 19 4 -1 -4 63707.1 990.522 5 4 -1 -4 66410.3 1224.93 3 4 -1 -3 45858.5 945.207 3 4 -1 -3 43597.5 870.272 23 -4 1 3 44254.6 921.992 19 4 -1 -2 125010. 1751.09 23 -4 1 2 129547. 1765.19 19 4 -1 -2 130655. 1793.93 3 -4 1 1 19919.9 574.880 19 4 -1 -1 20945.9 596.292 3 4 -1 0 92174.0 1529.46 23 4 -1 0 91705.2 1463.90 3 4 -1 1 41516.0 978.240 23 -4 1 -1 41537.9 905.942 19 4 -1 1 41216.1 935.000 3 -4 1 -1 42389.9 839.767 21 -4 1 -2 80370.4 1418.12 19 -4 1 -2 80985.9 1323.90 21 -4 1 -2 83261.5 1462.69 1 4 -1 2 83649.5 1483.96 3 -4 1 -3 102409. 1781.28 1 -4 1 -3 100968. 1627.79 21 -4 1 -3 97604.3 1704.84 19 4 -1 4 4385.89 353.633 22 -4 1 -4 4917.45 329.783 21 -4 1 -4 4818.94 354.032 19 -4 1 -4 4974.91 372.829 1 -4 1 -5 81264.0 1605.99 21 4 -1 5 80847.1 1734.15 22 -4 1 -5 79844.5 1695.87 19 -4 1 -5 83433.7 1742.85 1 4 -1 6 5135.60 426.616 22 -4 1 -6 5179.85 391.670 21 -4 1 -6 5898.79 453.508 1 4 -1 7 49679.1 1449.17 22 -4 1 -7 46149.3 1263.04 21 4 -1 7 48456.5 806.834 10 4 -1 7 47970.0 841.991 15 -4 1 -7 47668.7 1400.61 1 4 -1 8 659.414 89.2223 10 4 -1 8 790.148 104.347 15 4 -1 9 50662.4 829.050 10 4 -1 9 51119.5 883.595 15 4 -1 10 905.202 94.2093 10 4 -1 10 1058.36 112.124 15 4 -1 11 21099.6 462.070 15 4 -1 11 21304.6 426.729 10 -4 1 -12 236.467 39.1786 7 4 -1 12 236.545 38.2244 10 4 -1 12 168.792 45.3246 15 4 -1 13 10680.5 222.822 15 4 0 -15 4052.64 158.147 6 4 0 -15 4010.79 163.641 12 -4 0 15 4040.65 152.375 15 4 0 -14 5279.24 207.187 6 4 0 -14 5182.72 214.668 12 -4 0 14 5079.56 201.501 15 4 0 -14 4702.40 183.867 14 4 0 -13 179.411 50.7544 12 4 0 -13 194.252 58.9549 6 -4 0 13 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3 4 0 -4 4349.11 219.996 5 4 0 -3 197642. 2451.30 3 4 0 -3 197995. 2166.16 5 4 0 -2 34796.7 784.402 3 4 0 -2 33935.0 598.250 5 -4 0 2 35724.6 790.272 19 -4 0 1 307820. 3465.49 19 4 0 -1 315725. 3534.95 3 -4 0 0 7837.52 349.520 19 4 0 0 8782.94 398.785 3 -4 0 -1 43510.8 905.349 21 -4 0 -1 42602.0 917.531 19 -4 0 -1 44257.8 963.655 1 4 0 1 43740.3 994.206 3 4 0 1 42236.1 741.957 4 4 0 2 16994.7 624.892 22 -4 0 -2 17137.7 579.650 21 -4 0 -2 17152.1 578.606 19 -4 0 -2 18106.0 634.710 1 4 0 2 18367.7 640.899 3 4 0 3 6256.52 398.868 22 -4 0 -3 6367.07 373.463 21 -4 0 -3 6118.33 396.557 1 -4 0 -3 6175.44 371.182 19 -4 0 -4 3687.66 320.545 21 -4 0 -4 3865.48 315.381 19 4 0 4 3962.26 342.736 22 -4 0 -4 3929.78 341.801 1 -4 0 -5 8132.99 490.718 21 4 0 5 8145.39 524.694 22 -4 0 -5 8984.79 543.558 1 4 0 6 88086.4 1958.66 22 4 0 6 90129.5 1212.70 10 4 0 6 86209.0 1223.86 15 -4 0 -6 89936.5 1958.83 1 4 0 7 306.569 132.570 22 -4 0 -7 363.553 125.694 21 -4 0 -7 288.450 134.191 1 4 0 7 315.386 64.7325 10 4 0 7 613.770 91.9513 15 4 0 8 46274.1 800.587 10 4 0 8 46073.9 832.922 15 4 0 9 667.132 86.8876 10 4 0 9 510.002 83.3055 15 4 0 10 43046.1 746.205 15 4 0 10 44193.5 717.973 10 4 0 11 12.8571 32.6417 10 4 0 11 64.3801 39.2023 15 4 0 12 9675.10 214.182 10 4 0 12 9637.98 238.662 15 4 1 -16 17806.8 323.028 6 4 1 -15 1140.22 91.1311 12 4 1 -15 946.349 84.4617 6 -4 -1 15 1059.70 79.8871 15 4 1 -15 1043.19 77.5527 14 4 1 -14 3391.48 175.548 6 4 1 -14 3298.40 174.142 12 -4 -1 14 3496.48 166.123 15 4 1 -14 3378.32 160.331 14 4 1 -13 13225.3 382.982 12 4 1 -13 13346.8 380.382 6 -4 -1 13 13571.1 373.064 15 4 1 -12 3266.89 188.537 12 4 1 -12 3405.07 194.729 6 4 1 -12 3423.84 210.542 16 -4 -1 12 3470.13 190.405 15 4 1 -11 75425.7 1105.89 12 4 1 -11 76477.6 1126.28 6 4 1 -11 76835.4 1165.32 16 -4 -1 11 78619.5 1115.90 15 -4 -1 10 649.916 152.071 20 4 1 -10 737.469 94.6863 6 4 1 -10 733.118 93.8997 16 4 1 -10 914.561 183.509 5 -4 -1 9 67052.0 1467.52 20 4 1 -9 70181.8 1468.17 3 4 1 -9 71173.5 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5371.14 340.621 3 -4 -1 -1 4761.11 301.464 21 4 1 2 243966. 3188.97 22 -4 -1 -2 241749. 3112.63 21 -4 -1 -2 246586. 3009.31 19 -4 -1 -2 249650. 3197.63 1 -4 -1 -3 4356.48 329.959 21 4 1 3 4841.00 366.544 22 -4 -1 -3 4433.57 311.006 19 -4 -1 -3 4306.01 345.369 1 -4 -1 -4 50131.9 1292.19 21 4 1 4 51823.1 1349.01 22 -4 -1 -4 50675.5 1196.20 19 -4 -1 -4 52339.0 1331.76 1 -4 -1 -5 25878.6 961.879 1 -4 -1 -5 22769.4 895.429 21 4 1 5 25678.0 971.970 22 -4 -1 -6 4003.71 388.671 1 4 1 6 3186.71 356.494 22 -4 -1 -6 3239.83 346.613 21 4 1 6 3463.82 196.377 15 4 1 7 40897.5 751.569 10 4 1 7 38888.0 747.496 15 4 1 8 5252.28 240.924 10 4 1 8 5104.66 246.605 15 4 1 9 27076.7 556.663 10 4 1 9 25944.1 562.360 15 4 1 10 2512.38 144.243 10 4 1 10 2461.87 146.307 15 4 1 11 23040.1 412.831 10 4 1 11 21766.8 413.116 15 -4 -1 -12 34.4425 20.5670 7 4 1 12 82.6586 24.1447 10 4 1 12 29.3050 22.0861 15 4 2 -17 37619.2 474.355 18 4 2 -16 554.129 58.6360 6 4 2 -16 478.320 46.9744 14 4 2 -15 12870.1 325.264 6 4 2 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5475.92 250.613 9 4 6 0 5666.76 276.780 17 4 6 0 5043.10 245.503 8 4 6 1 370.866 126.733 22 4 6 1 550.474 172.897 4 4 6 1 391.776 90.7627 17 4 6 1 383.958 68.2061 9 -4 -6 -1 318.256 134.715 21 4 6 1 510.754 88.7737 8 4 6 2 409.599 90.0506 17 4 6 2 457.349 78.7934 9 4 6 2 509.658 91.4129 8 4 6 3 19180.2 450.267 9 4 6 3 19488.4 540.831 17 4 6 3 19830.2 520.423 8 4 6 4 298.105 73.5808 17 4 6 4 193.297 62.6622 8 4 6 5 26560.6 548.758 10 4 6 5 26788.8 579.324 17 4 6 5 27944.1 576.823 8 4 6 6 632.610 74.3134 10 4 6 6 525.917 69.9292 17 4 6 6 601.865 72.7820 8 4 6 7 38688.1 589.202 10 4 6 7 39622.2 585.013 8 4 6 8 359.161 42.0474 10 4 6 8 293.369 33.1065 8 4 7 -16 5395.53 167.682 18 4 7 -16 5794.14 172.220 14 4 7 -15 1445.32 100.418 18 4 7 -15 1526.53 103.204 14 4 7 -14 29974.9 562.863 18 4 7 -14 30781.2 567.993 14 4 7 -13 376.609 68.1865 18 4 7 -13 343.352 68.2418 14 4 7 -12 77998.5 1162.69 11 4 7 -12 78686.1 1145.85 14 4 7 -11 2182.67 164.955 11 4 7 -11 1945.29 145.504 18 4 7 -11 1928.41 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176.606 94.2276 21 5 5 1 184.616 68.7291 17 5 5 1 180.077 54.7401 9 5 5 1 160.660 64.8720 8 5 5 2 26663.6 570.808 10 5 5 2 27110.3 565.713 9 5 5 2 25553.5 625.152 17 5 5 2 27019.5 619.430 8 5 5 3 70.6627 45.4155 10 5 5 3 75.0993 52.3382 17 5 5 3 193.093 57.7900 9 5 5 3 105.231 54.9737 8 5 5 4 68641.4 1044.18 17 5 5 4 70659.4 1064.16 8 5 5 5 1493.83 124.602 10 5 5 5 1524.75 122.193 8 5 5 6 57984.3 841.341 10 5 5 6 58665.4 819.625 8 5 5 7 3080.89 139.197 10 5 5 7 3113.04 124.975 8 5 5 8 8734.75 196.198 10 5 6 -16 1534.42 74.6696 6 5 6 -16 1461.02 78.9506 18 5 6 -16 1626.35 85.0450 14 5 6 -15 33203.3 503.238 6 5 6 -15 31853.6 518.838 18 5 6 -15 32851.0 530.851 14 5 6 -14 352.067 55.8520 18 5 6 -14 380.655 55.9486 6 5 6 -14 405.171 63.7003 14 5 6 -13 42467.2 723.370 11 5 6 -13 42228.3 681.359 6 5 6 -13 41582.6 701.401 18 5 6 -13 43468.7 729.273 14 5 6 -12 10483.1 341.891 11 5 6 -12 9773.37 303.035 6 5 6 -12 9993.27 324.628 14 5 6 -11 33080.2 617.902 6 5 6 -11 34340.2 659.612 14 5 6 -10 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8 10 5 -4 20355.1 357.756 11 10 5 -4 22751.0 384.518 8 10 5 -3 1040.03 70.5201 8 10 6 -9 17118.8 292.964 11 10 6 -8 3412.45 124.115 11 10 6 -7 20312.7 341.082 11 10 6 -6 2604.79 103.858 11 11 -5 -2 9841.24 222.737 24 11 -4 -5 20886.7 340.818 16 11 -4 -4 149.849 33.8382 16 11 -4 -3 11856.2 276.798 24 11 -4 -3 11290.5 246.994 16 11 -4 -2 3662.69 145.207 24 11 -4 -2 3242.61 123.253 16 11 -4 -1 11871.8 257.577 24 11 -4 -1 11701.2 236.477 16 11 -3 -6 11120.5 234.404 16 11 -3 -5 6452.17 180.280 16 11 -3 -4 7946.29 235.315 24 11 -3 -4 7642.09 180.262 6 11 -3 -4 7576.65 202.273 16 11 -3 -3 3681.01 157.484 24 11 -3 -3 3631.41 121.140 6 11 -3 -3 3550.78 135.390 16 11 -3 -2 1742.03 104.537 24 11 -3 -2 1689.57 81.5059 6 11 -3 -2 1500.86 85.7190 16 11 -3 -1 1323.17 83.4662 24 11 -3 -1 1350.43 68.7047 6 11 -3 -1 1107.94 68.8546 16 11 -3 0 2993.58 106.639 11 11 -2 -7 3486.59 115.229 6 11 -2 -7 3845.89 131.434 8 11 -2 -6 23670.4 371.394 6 11 -2 -6 24239.9 387.179 8 11 -2 -5 26527.1 413.953 6 11 -2 -5 26349.3 411.636 8 11 -2 -4 23079.0 370.051 11 11 -2 -4 26017.7 409.507 6 11 -2 -4 22139.2 382.277 16 11 -2 -4 24548.2 381.197 8 11 -2 -3 15219.1 334.114 24 11 -2 -3 14575.1 289.673 11 11 -2 -3 15946.8 304.504 6 11 -2 -3 13935.9 282.807 16 11 -2 -2 8008.37 218.478 24 11 -2 -2 8362.63 211.083 11 11 -2 -1 4457.59 149.738 11 11 -2 -1 5398.88 155.734 6 11 -2 0 223.317 34.4751 11 11 -2 0 347.691 38.7760 6 11 -1 -8 363.992 40.6925 6 11 -1 -8 452.887 48.3608 8 11 -1 -7 13749.0 274.917 6 11 -1 -7 13943.4 285.267 8 11 -1 -6 14579.0 297.289 6 11 -1 -6 14901.4 304.468 8 11 -1 -5 10611.6 233.594 11 11 -1 -5 11313.8 261.236 6 11 -1 -5 11079.7 256.615 8 11 -1 -4 19482.8 353.060 11 11 -1 -4 19688.4 364.665 6 11 -1 -4 18917.4 343.752 8 11 -1 -3 18661.7 353.033 11 11 -1 -3 18284.3 316.936 8 11 -1 -2 12033.0 270.756 11 11 -1 -2 11917.0 262.662 6 11 -1 -1 5298.30 163.616 11 11 -1 -1 5375.20 160.579 6 11 -1 0 1862.39 86.0872 11 11 -1 0 2556.39 97.9789 6 11 0 -9 3356.49 111.835 6 11 0 -9 3440.34 114.005 8 11 0 -8 10631.3 231.089 6 11 0 -8 10632.1 235.807 8 11 0 -7-27.0068 29.3582 6 11 0 -7 42.0819 29.5088 8 11 0 -6 13481.5 267.171 11 11 0 -6 13794.8 292.402 6 11 0 -6 14085.0 297.982 8 11 0 -5 4890.71 161.832 11 11 0 -5 4605.05 163.358 6 11 0 -5 4631.70 162.476 8 11 0 -4 9111.75 235.212 11 11 0 -4 8610.72 226.832 6 11 0 -4 8409.57 218.921 8 11 0 -3 14475.5 304.271 11 11 0 -3 13990.3 294.391 6 11 0 -3 13820.6 272.013 8 11 0 -2 12543.6 274.221 11 11 0 -2 13242.1 274.362 6 11 0 -1 8870.89 207.515 11 11 0 -1 9421.19 210.065 6 11 1 -9 6436.14 161.991 6 11 1 -9 6465.38 159.117 8 11 1 -8 6792.17 180.788 6 11 1 -8 6640.38 179.072 8 11 1 -7 5553.01 155.094 11 11 1 -7 5712.06 172.831 6 11 1 -7 6048.81 179.367 8 11 1 -6 34.5170 25.2842 11 11 1 -6 14.2748 25.8452 6 11 1 -6 20.8413 31.0993 8 11 1 -5 2667.17 120.598 11 11 1 -5 2680.03 121.740 6 11 1 -5 2709.50 123.322 8 11 1 -4 3334.56 137.206 11 11 1 -4 3026.23 127.274 6 11 1 -4 3220.16 129.498 8 11 1 -3 6418.93 187.086 11 11 1 -3 6191.73 178.551 6 11 1 -3 6027.34 166.855 8 11 1 -2 12749.5 256.515 11 11 1 -2 11607.9 238.925 6 11 2 -8 3415.20 118.270 6 11 2 -8 3409.29 120.149 8 11 2 -7 4812.85 147.568 6 11 2 -7 5039.73 155.815 8 11 2 -6 6277.89 179.926 11 11 2 -6 6470.17 176.259 6 11 2 -6 6436.04 183.632 8 11 2 -5 78.5554 30.9121 11 11 2 -5 30.9281 23.6640 6 11 2 -5 8.95902 25.1890 8 11 2 -4 8907.18 219.128 11 11 2 -4 8964.95 202.958 6 11 2 -4 9025.35 213.341 8 11 2 -3 6039.76 164.707 11 11 2 -3 5898.23 153.863 8 11 3 -7 12378.8 242.092 11 11 3 -7 13072.9 243.582 8 11 3 -6 7328.01 185.868 11 11 3 -6 7876.40 187.130 8 11 3 -5 4725.36 144.756 11 11 3 -5 5003.88 145.033 8 0 0 0 0.00 0.00 0 TITL absorption in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 9.140913 11.360011 13.822266 109.3657 105.2607 93.4619 ZERR 2.00 0.000276 0.000283 0.000404 0.0024 0.0027 0.0023 LATT 1 SFAC C H N O P Pd UNIT 64.00 60.00 2.00 4.00 2.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 35226